超声提取-离子色谱法测定银精矿中水溶性氟
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摘要
银精矿中水溶性氟会随雨水的冲刷进入生物圈,直接对土壤、水体、大气、人类健康产生危害。实验提出超声提取-离子色谱法测定银精矿中水溶性氟,为银精矿中水溶性氟的检测及后续环境影响评估提供重要的技术支撑。称取0.2g样品(过150目筛),加入30mL水,在40℃时超声提取20min后,使用阴离子交换柱进行分离,使用碳酸钠-碳酸氢钠混合溶液作为淋洗液进行淋洗,洗脱时间为25min,通过电导检测器进行F-检测。F-质量浓度在0.5～10mg/L范围内与对应的峰面积呈线性关系,校准曲线线性相关系数为0.999 8;方法检出限为0.062mg/L,测定下限为0.21mg/L。按照实验方法测定两个银精矿中水溶性氟,测定结果的相对标准偏差(RSD,n=6)为3.8%和4.3%;加标回收率为92%～102%。
The water-soluble fluoride(F-)in silver concentrate can enter into biosphere with rainwash and directly cause harm to the soil,water system,atmosphere and human being.The determination of watersoluble fluoride in silver concentrate by ultrasonic extraction-ion chromatography was proposed.It provided important technical support for the detection of water-soluble fluoride in silver concentrate and subsequent environmental impact assessment.0.2 g of sample(passing through 150-mesh sieve)was added into 30 mL of water.After ultrasonic extraction at 40℃ for 20 min,the anion exchange column was employed for separation.The mixture solution of sodium carbonate-sodium bicarbonate was used as leacheate for elution.The elution time was 25 min.The content of water-soluble fluoride was detected by electrical conductivity detector.The mass concentration of F-in range of 0.5-10 mg/L was linear to the corresponding peak area.The linear correlation coefficient of calibration curve was 0.999 8.The detection limit was 0.062 mg/L and the low limit of determination was 0.21 mg/L.The content of water-soluble fluoride in two silver concentrate samples was determined according to the experimental method.The relative standard deviation(RSD,n=6)of determination results was 3.8% and 4.3%,respectively.The recoveries were between 92% and 102%.
The water-soluble fluoride(F-)in silver concentrate can enter into biosphere with rainwash and directly cause harm to the soil,water system,atmosphere and human being.The determination of watersoluble fluoride in silver concentrate by ultrasonic extraction-ion chromatography was proposed.It provided important technical support for the detection of water-soluble fluoride in silver concentrate and subsequent environmental impact assessment.0.2 g of sample(passing through 150-mesh sieve)was added into 30 mL of water.After ultrasonic extraction at 40℃ for 20 min,the anion exchange column was employed for separation.The mixture solution of sodium carbonate-sodium bicarbonate was used as leacheate for elution.The elution time was 25 min.The content of water-soluble fluoride was detected by electrical conductivity detector.The mass concentration of F-in range of 0.5-10 mg/L was linear to the corresponding peak area.The linear correlation coefficient of calibration curve was 0.999 8.The detection limit was 0.062 mg/L and the low limit of determination was 0.21 mg/L.The content of water-soluble fluoride in two silver concentrate samples was determined according to the experimental method.The relative standard deviation(RSD,n=6)of determination results was 3.8% and 4.3%,respectively.The recoveries were between 92% and 102%.
引文
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[3]肖健秋,杨建洪,黄建军,等.地方性氟中毒病区人群氟性骨损伤致病风险评价[J].实用预防医学,2014,21(11):1313-1316.XIAO Jian-qiu,YANG Jian-hong,HUANG Jian-jun,et al.Evaluation on the risk of fluoride bone injury among the population in endemic fluorosis area[J].Practical Preventive Medicine,2014,21(11):1313-1316.
[4]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 3884.5-2012铜精矿化学分析方法氟量的测定[S].北京:中国标准出版社,2013.
[5]窦怀智,陆彩霞,侯晋.离子色谱法测定镍矿中氟和氯[J].冶金分析,2012,32(8):59-62.DOU Huai-zhi,LU Cai-xia,HOU Jin.Determination of fluoride and chloride in nickel ore by ion chromatography[J].Metallurgical Analysis,2012,32(8):59-62.
[6]李颖娜,徐志彬,张志伟.高温水解-离子色谱法测定铁矿石中氟和氯[J].冶金分析,2016,36(6):23-28.LI Ying-na,XU Zhi-bin,ZHANG Zhi-wei.Determination of fluoride and chloride in iron ores by pyrohydrolysisionchromatography[J].Metallurgical Analysis,2016,36(6):23-28.
[7]Banjoo D R,Nelson R K.Improved ultrasonic extraction procedure for the determination of polycyclic aromatic hydrocarbons in sediments[J].Journal of Chromatography A,2005(1):9-18.
[8]Navarro P,Etxebarria N,Arana G.Development of a focused ultrasonic-assisted extraction of polycyclic aromatic hydrocarbons in marine sediment and mussel samples[J].Analytica Chimica Acta,2009(2):178-182.
[9]甘志勇,农耀京,彭靖茹,等.超声提取-石墨炉原子吸收光谱法测定土壤中有效态镉[J].理化检验:化学分册,2013,49(11):1315-1317.GAN Zhi-yong,NONG Yao-jing,PENG Jing-ru,et al.Ultrosonic extration-GF-AAS determination of available cadmium in soil[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2013,49(11):1315-1317.
[10]Tian K,Ca1as J E,Dasgupta P K,et al.Preconcentration/preelution ion chromatography for the determination of perchlorate in complex samples[J].Talanta,2005,65(3):750-755.
[11]刘欣,李晶,米其利,等.离子色谱法测定变质烟用浸膏中硫化氢的含量[J].理化检验:化学分册,2018,54(7):761-765.LIU Xin,LI Jing,MI Qi-li,et al.Determiantion of hydrogen sulfide in deteriorated extracts for tobacco by ion chromatography[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2018,54(7):761-765.